CN103588856A - Method for extracting peanut oil and fat and protein with ultrasonic assisted aqueous enzymatic method - Google Patents

Method for extracting peanut oil and fat and protein with ultrasonic assisted aqueous enzymatic method Download PDF

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CN103588856A
CN103588856A CN201310557567.4A CN201310557567A CN103588856A CN 103588856 A CN103588856 A CN 103588856A CN 201310557567 A CN201310557567 A CN 201310557567A CN 103588856 A CN103588856 A CN 103588856A
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peanut
emulsion
protein
oil
milk sap
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CN103588856B (en
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杨瑞金
张文斌
迟延娜
赵伟
华霄
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Jiangsu Jun Kai biological Polytron Technologies Inc
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Jiangnan University
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Abstract

The invention discloses a method for extracting peanut oil and fat and protein with an ultrasonic assisted aqueous enzymatic method, belonging to the technical field of fine processing of agricultural products and comprehensive utilization of by-products. The method comprises the following steps: after grinding blanched peanuts with a dry method, adding water to adjust alkali for ultrasonic-assisted extraction, and digesting after adjusting alkali at the second time; low-speed centrifuging to obtain free oil I and emulsion I, and high-speed centrifuging the emulsion I to obtain free oil II and emulsion II; causing the emulsion II to carry out complex enzyme breaking to obtain demulsification oil I, and causing stubborn emulsion to carry out ethanol-assisted breaking to obtain demulsification oil II; ultra-filtering and desalting protein fluid, and then spray drying to obtain peanut isolate protein powder. Finally, the extraction ratio of free oil is 83 percent, the extraction ratio of total oil is 92 percent, the protein recovery ratio is 91.6 percent, the peanut protein purity is 89 percent, and the breaking ratio of emulsion can achieve 97-98 percent. Compared with the traditional aqueous enzymatic method, the method has the advantages that the extraction ratio of free oil is increased, the dosage of enzyme is greatly reduced, the residual oil ratio of emulsion is significantly reduced, and meanwhile, the peanut protein powder with high purity and good functionality is obtained.

Description

A kind of ultrasonic auxiliary water Enzymatic Extraction peanut grease and method of protein
Technical field
The present invention relates to a kind of ultrasonic auxiliary water Enzymatic Extraction peanut grease and method of protein, belong to agricultural-food retrofit and byproduct comprehensive thereof and utilize technical field.
Technical background
Peanut is the valuable source of mankind's edible fats and protein.The tradition of peanut is utilized mode take and is squeezed or leach and get oil as main, though traditional method has the advantage that grease extraction yield is high, but Semen arachidis hypogaeae protein (dregs of rice) is generally used as feed, cause protein resource serious waste on the one hand, also to environment, bring larger pressure on the other hand.Continuous enhancing along with people's environmental consciousness, and population increase brings the great demand to protein resource, the comprehensive exploitation to quality plant albumen, the especially exploitation to peanut resource, not only there is higher health and be worth, also there is very high environment and economy benefit.
Aqueous enzymatic method is as a kind of novel oil extracting methods, it be take machinery and enzymolysis and is means destruction plant cell wall, in leaching process without the need for machine solvent, the grease extracting does not need Degumming Procedures, reduce cost of investment and energy expenditure, and in putting forward oily process, can remove the poisonous or antinutritional factor in some oil plants.In addition, when extracting grease, protein (or its hydrolysate) and carbohydrate in energy efficient recovery raw material.Patent CN1419837A has reported a kind of method of utilizing prozyme (cellulase, polygalacturonase and neutral protease) to extract peanut oil and Semen arachidis hypogaeae protein, and grease yield is 94-96%, and protein yield is 73-75%.2005, Wang Yingyao utilized aqueous enzymatic method to extract peanut grease and protolysate simultaneously, and the milk sap generating in technique has been carried out property analysis and abolished research, and result shows that the highest yield of grease and protolysate reaches respectively 92.2% and 82.5%.2006, Hua Di etc. adopted Alcalase hydrolysis peanut, by a step enzyme digestion reaction, can extract 79.32% free oil and 71.38% protolysate.To the slag of technique gained and milk sap, select neutral protease As1398 to carry out secondary enzymolysis, final total free oil yield can reach 91.98%, and total yield of aminosal can reach 88.21%.Within 2010, river profit China utilizes grease and protein in aqueous enzymatic extraction band skin peanuts and decortication peanut, and carried out pilot scale amplification test, grease extraction yield is respectively 79.68% (band skin peanuts) and 81.95% (decortication peanut), and yield of aminosal reaches respectively 73.05% (band skin peanuts) and 72.20% (decortication peanut).Every qualities such as its color and luster of the peanut oil that pilot process obtains, peroxide value, acid number reach the standard of three grades of peanut oil of country substantially.Although traditional aqueous enzymatic method obtains higher grease and protein extracting ratio, due to a large amount of uses of enzyme, production cost is increased, and protein become bitter peptides by enzymolysis, apply limited.
In recent years, although aqueous enzymatic method extracts the research person's of being studied much of peanut grease and protolysate concern simultaneously, traditional aqueous enzymatic method is proposed a large amount of uses of enzyme in oily process and is made production cost higher.And free oil is low in the auxiliary water method of emerging enzyme, and the milk sap forming can not well be abolished, and residual oil content is high, thereby greatly limited aqueous enzymatic method, is applied to suitability for industrialized production.Therefore, develop a kind of suitability for industrialized production that is applicable to, and can be simultaneously significant with higher extracted rate extraction peanut grease and method of protein.
Summary of the invention
The problems such as body of the present invention provides a kind of ultrasonic auxiliary water Enzymatic Extraction peanut grease and method of protein, has solved traditional method free oil extraction yield low, and in milk sap the comprehensive utilization of the high and protein of residual oil content is not enough, technical scheme is as follows:
(1) decortication peanut is carried out to dry ground, add after water is adjusted alkali and carry out supersound process;
(2) adjust pH, after carrying with water-bath alkali, low-speed centrifugal obtains free oil I, milk sap I, protein liquid and slag;
(3) will after the dilution of the protein liquid in step (2), carry out ultrafiltration, get trapped fluid spraying and be dried, obtain separating protein powder of peanut, milk sap I is carried out obtaining free oil II and milk sap II after high speed centrifugation;
(4) utilize aqueous enzymatic method to carry out enzyme process breakdown of emulsion to the milk sap II in step (3), after the enzyme that goes out, obtain breakdown of emulsion oil I and obstinate milk sap;
(5) utilize ethanol to assist and abolish the obstinate milk sap in step (4), obtain breakdown of emulsion oil II.
In order to reach better effect, step (1) utilizes medicinal herb grinder to carry out dry ground peanut, and median size is controlled at 20~50 μ m.Peanut after pulverizing is by solid-liquid ratio 1:2~1:6(w/v) be dissolved in water, with NaOH, be adjusted to alkalescence.Ultrasonic power 300W-500W, ultrasonic time 2-5min.
In step (2), alkali is carried temperature 60 C, time 2-5h.
150 ℃~200 ℃ of the spray-dired inlet temperatures of step (3) protein liquid, 70 ℃~100 ℃ of temperature outs.
In step (4), the condition of enzyme process breakdown of emulsion is papoid and Phospholipid hydrolase (2:1, w/w), enzyme concentration 0.5%~2%(w/w), 40 ℃~60 ℃ of hydrolysis temperatures, enzymolysis time 2~4h, solid-liquid ratio 1:0.5~1:2(w/w).The enzyme condition of going out is: 80 ℃~100 ℃ of temperature, time 10~20min.
In step (5), ethanol breakdown of emulsion condition is concentration 20~60%(v/v), 0.5h~1h, solid-liquid ratio 1:1~1:3(v/v).
In addition the obstinate milk sap that cannot be abolished by enzyme is carried out to the auxiliary breakdown of emulsion of ethanol, make the residual oil content in milk sap lower.Realizing abolishing completely of milk sap, when percent of total oil increases significantly, Semen arachidis hypogaeae protein solution is being carried out to ultrafiltration desalination, can obtain that purity is higher, functional property is better, apply peanut protein isolate more fully.
Processing condition are:
(1) cleaning screening: remove impurity and moldy kernel in decortication blanched peanut;
(2) peanut is pulverized: adopt medicinal herb grinder that peanut is crushed to particle diameter at 20~50 μ m;
(3) ultrasound condition: ultrasonic power 300~500w, ultrasonic time 2~5min;
(4) alkali carry-centrifugal: peanut and water after pulverizing are carried out to mixed dissolution according to a certain percentage, with NaOH solution, system are adjusted to alkalescence, lixiviate 30~60min, after, again pH is recalled to alkalescence, lixiviate 2~5h, rear centrifugal layering obtains free oil I, milk sap I, protein liquid and slag;
(5) abolishing of milk sap: carry out enzyme process breakdown of emulsion after removing oil phase and water after milk sap high speed centrifugation, enzyme-added kind: papoid, Phospholipid hydrolase; Enzyme concentration: 0.5%~2%(w/w); Hydrolysis temperature: 50~70 ℃; Enzymolysis time: 3~5h.Centrifugation obtains part breakdown of emulsion oil, carries out abolishing of obstinate milk sap.Alcohol concn: 40~60%; Time: 1~2h; Solid-liquid ratio 1:1~1:3; Centrifugal that another part breakdown of emulsion is oily;
(6) the enzyme condition of going out: 80 ℃~100 ℃ of temperature; Time 10~30min;
(7) spraying is dry: protein liquid is sprayed dry, and 150 ℃~200 ℃ of inlet temperatures, 70~100 ℃ of temperature outs, obtain peanut protein isolate.
Analytical procedure is:
Crude fat is measured: Soxhlet extraction process
Crude protein is measured: triumphant formula nitriding (N=5.46)
Oleaginousness * 100% in demulsification efficiency=(breakdown of emulsion oil I+breakdown of emulsion oil II)/raw material
Oleaginousness * 100% in free oil yield=(free oil I+free oil II)/raw material
Total oily yield=(free oil I+free oil II+breakdown of emulsion oil I+breakdown of emulsion oil II)) oleaginousness * 100% in/raw material
Beneficial effect of the present invention: the present invention for traditional physical and chemical process, does not use organic reagent with biological processing technology generations, and equipment and technology is simple, significantly reduces the energy and resource consumption.Relatively traditional aqueous enzymatic method technique, the present invention utilizes the effect of ultrasonic mechanical vibration, to Mierocrystalline cellulose, starch, the macromolecular substance such as protein carry out mechanicalness scission of link, promote separating out of grease in peanut, and the extraction yield of free oil is significantly increased.And select the papoid of multidigit point and Phospholipid hydrolase is compound that the milk sap forming in peanut grease and proteins extraction process is abolished, greatly reduced the consumption of enzyme, reduce production costs, and avoided proteolysis to become bitter taste small peptide.Purity through the peanut protein of ultrafiltration desalination is higher, and emulsifying property, whipability, retentiveness and to hold the functional propertys such as oiliness better, has promoted the comprehensive utilization of protein.The present invention also and the obstinate milk sap that cannot abolish enzyme process carry out that ethanol is auxiliary to be abolished, the rate of abolishing of milk sap is improved greatly, obtain higher percent of total oil.
Accompanying drawing explanation
Fig. 1: the auxiliary water method of enzyme is extracted peanut grease and protein process route chart simultaneously
Embodiment
Embodiment 1
The peanut screening and removing impurities of peeling, dry ground to peanut median size is 38 μ m left and right, peanut paste and water after pulverizing are pressed to 1:5(w/v) solid-liquid ratio dissolving, after the pH of system being adjusted to 9.00 with 1M NaOH, adopt the ultrasonic echography 3min of 400W, and then pH is adjusted to after 9.00,60 ℃ of water-bath lixiviate 4h to 3000 is divided into four layers after leaving heart 20min, be respectively free oil I, milk sap I, protein liquid and slag, weigh the quality of free oil I.After protein liquid dilution, selecting molecular weight cut-off is that the film of 10k carries out ultrafiltration, gets trapped fluid spraying dry, 170 ℃ of inlet temperatures, 80 ℃ of temperature outs.Milk sap I is carried out to 8000 and leave heart 20min, obtain free oil II, weigh its quality.Remaining emulsus liquid phase is carried out to enzyme process and abolish, condition is: papoid/Phospholipid hydrolase (2:1, w/w), temperature 60 C, enzyme concentration 1.5% (w/w), enzymolysis time 4h, 95 ℃ of enzyme-removal temperatures, time 15min, rear centrifugal 5000 turn part breakdown of emulsion oil and the obstinate milk sap of 15min.Obstinate milk sap mixes by the solid-liquid ratio of 1:1 with 50% ethanol, slowly stirs 30min, and centrifugal 5000 turn 15min, obtain breakdown of emulsion oil, weighs the quality of breakdown of emulsion oil.
Free oil extraction yield is 82%, and percent of total oil is 93%, and protein recovery is 90.6%, and Semen arachidis hypogaeae protein purity is 88%.
Can be up to 97%~98% in conjunction with the rate of abolishing of enzyme process and the auxiliary milk sap of ethanol in the present invention.
Through local flavor, measure, the peanut protein isolate of gained of the present invention is almost without bitter taste.
Through functional property, measure, the peanut protein isolate of gained of the present invention is in emulsifying property, whipability, retentiveness and hold the albumen that is all significantly better than traditional aqueous enzymatic method technique gained aspect oiliness.
Embodiment 2
The peanut screening and removing impurities of peeling, dry ground to peanut median size is 40 μ m left and right, peanut paste and water after pulverizing are pressed to 1:4(w/v) solid-liquid ratio dissolving, with 1M NaOH, the pH of system is adjusted to 8.50, the ultrasonic echography 4min of rear employing 450W, after pH recalled to after 8.50,60 ℃ of water-bath lixiviate 5h to 3000 be divided into four layers after leaving heart 20min, be respectively free oil I, milk sap I, protein liquid and slag, weigh the quality of free oil I.After protein liquid dilution, selecting molecular weight cut-off is that the film of 10k carries out ultrafiltration, gets trapped fluid spraying dry, 180 ℃ of inlet temperatures, 90 ℃ of temperature outs.Milk sap I is carried out to 7000 and leave heart 20min, obtain free oil II, weigh its quality.Remaining emulsus liquid phase is carried out to enzyme process and abolish, condition is: papoid/Phospholipid hydrolase (2:1, w/w), 55 ℃ of temperature, enzyme concentration 1% (w/w), enzymolysis time 4h, 95 ℃ of enzyme-removal temperatures, time 15min, rear centrifugal 5000 turn part breakdown of emulsion oil and the obstinate milk sap of 15min.Obstinate milk sap mixes by the solid-liquid ratio of 1:2 with 40% ethanol, slowly stirs 30min, and centrifugal 5000 turn 15min, obtain breakdown of emulsion oil, weighs the quality of breakdown of emulsion oil.
Free oil extraction yield is 83%, and percent of total oil is 92%, and protein recovery is 91.6%, and Semen arachidis hypogaeae protein purity is 89%.
Can be up to 97%~98% in conjunction with the rate of abolishing of enzyme process and the auxiliary milk sap of ethanol in the present invention.
Through local flavor, measure, the peanut protein isolate of gained of the present invention is almost without bitter taste.
Through functional property, measure, the peanut protein isolate of gained of the present invention is in emulsifying property, whipability, retentiveness and hold the albumen that is all significantly better than traditional aqueous enzymatic method technique gained aspect oiliness.

Claims (10)

1. ultrasonic auxiliary water Enzymatic Extraction peanut grease and a method of protein, is characterized in that, step is as follows:
(1) decortication peanut is carried out to dry ground, add after water is adjusted alkali and carry out supersound process;
(2) adjust pH to alkalescence, after carrying with water-bath alkali, low-speed centrifugal obtains free oil I, milk sap I, protein liquid and slag;
(3) will after the dilution of the protein liquid in step (2), carry out ultrafiltration, get trapped fluid spraying and be dried, obtain separating protein powder of peanut, milk sap I is carried out obtaining free oil II and milk sap II after high speed centrifugation;
(4) utilize aqueous enzymatic method to carry out enzyme process breakdown of emulsion to the milk sap II in step (3), after the enzyme that goes out, obtain breakdown of emulsion oil I and obstinate milk sap;
(5) utilize ethanol to assist and abolish the obstinate milk sap in step (4), obtain breakdown of emulsion oil II.
2. method according to claim 1, is characterized in that, described step (1) utilizes medicinal herb grinder to carry out dry ground peanut, and median size is controlled at 20~50 μ m.
3. method according to claim 1, is characterized in that, described step (1) by the peanut after pulverizing by solid-liquid ratio 1:2~1:6(w/v) be dissolved in water, with NaOH, be adjusted to alkalescence.
4. method according to claim 1, is characterized in that, ultrasonic power 300W-500W in described step (1), ultrasonic time 2-5min.
5. method according to claim 1, is characterized in that, in described step (2), alkali is carried temperature 60 C, time 2-5h.
6. method according to claim 1, is characterized in that, 150~200 ℃ of the spray-dired inlet temperatures of described step (3) protein liquid, 70 ℃~100 ℃ of temperature outs.
7. method according to claim 1, is characterized in that, in described step (4), the condition of enzyme process breakdown of emulsion is papoid and Phospholipid hydrolase (2:1, w/w), enzyme concentration 0.5%~2%(w/w), 40 ℃~60 ℃ of hydrolysis temperatures, enzymolysis time 2~4h, solid-liquid ratio 1:0.5~1:2(w/w).
8. method according to claim 1, is characterized in that, the enzyme condition of going out in described step (4) is: 80 ℃~100 ℃ of temperature, time 10~20min.
9. method according to claim 1, is characterized in that, in described step (5), ethanol breakdown of emulsion condition is concentration 20~60%(v/v), 0.5h~1h, solid-liquid ratio 1:1~1:3(v/v).
10. according to method described in right 1-9, it is characterized in that, concrete steps are as follows:
(1) the peanut screening and removing impurities of peeling, dry ground to peanut median size is 40 μ m left and right, and peanut paste and water after pulverizing press to 1:4(w/v) solid-liquid ratio dissolving, with 1M NaOH, the pH of system is adjusted to 8.50, the rear ultrasonic echography 4min that adopts 450W;
(2) the peanut screening and removing impurities of peeling, dry ground to peanut median size is 40 μ m left and right, and peanut paste and water after pulverizing press to 1:4(w/v) solid-liquid ratio dissolving, with 1M NaOH, the pH of system is adjusted to 8.50, the rear ultrasonic echography 4min that adopts 450W;
(3) pH value of solution is recalled to after 8.50,60 ℃ of water-bath lixiviate 5h to 3000 and be divided into four layers after leaving heart 20min, be respectively free oil I, milk sap I, protein liquid and slag;
(4) by selecting molecular weight cut-off after the dilution of the described protein liquid of step (2), be that the film of 10k carries out ultrafiltration, get trapped fluid spraying dry, 170 ℃ of temperature outs, 90 ℃ of inlet temperatures, again milk sap I is carried out to 7000 and leave heart 20min, obtain free oil II and milk sap II;
(5) the described milk sap II of step (3) being carried out to enzyme process abolishes, condition is: papoid/Phospholipid hydrolase (2:1, w/w), 55 ℃ of temperature, enzyme concentration 1% (w/w), enzymolysis time 4h, 95 ℃ of enzyme-removal temperatures, time 15min, rear centrifugal 5000 turn 15min after breakdown of emulsion oil I and obstinate milk sap;
(6) the described obstinate milk sap of step (4) is mixed by the solid-liquid ratio of 1:2 with 40% ethanol, slowly stir 30min, centrifugal 5000 turn 15min, obtain breakdown of emulsion oil II.
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CN104479854A (en) * 2014-11-27 2015-04-01 江南大学 Method for extracting peanut oil and peanut protein simultaneously
CN106118855A (en) * 2016-06-27 2016-11-16 郭迎庆 A kind of method utilizing flaxseed to prepare edible oil
CN106701312A (en) * 2017-01-08 2017-05-24 山东乐悠悠花生油科技有限公司 Aqueous enzymatic method extraction process of high-quality peanut oil
CN106753766A (en) * 2017-01-08 2017-05-31 山东乐悠悠花生油科技有限公司 A kind of method of peanut oil and peanut protein based on the low aflatoxins of aqueous enzymatic extraction
CN107586594A (en) * 2017-09-27 2018-01-16 南京工业大学 Ethanol homogenization-assisted peony seed oil extraction method
CN108641804A (en) * 2018-04-13 2018-10-12 华侨大学 A kind of method of ultrasonic wave added aqueous enzymatic extraction setose abelmoschus seed oil and protein
CN109913312A (en) * 2019-04-10 2019-06-21 北京工商大学 A kind of emulsion breakdown method that aqueous enzymatic extraction Rice oil is formed
CN110106018A (en) * 2019-05-08 2019-08-09 西藏农牧学院 A kind of open country peach peach kernel grease microcapsule and preparation method thereof
CN111234919A (en) * 2020-01-19 2020-06-05 河南农业大学 Preparation method of functional peanut oil
CN111254005A (en) * 2020-01-19 2020-06-09 河南农业大学 Preparation method of functional edible oil
CN115812841A (en) * 2022-12-14 2023-03-21 中国农业科学院农产品加工研究所 Method for efficiently and synchronously separating oil and protein in peanut oil aqueous enzymatic preparation

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CN104026245A (en) * 2014-06-10 2014-09-10 江南大学 Low-fat peanut milk beverage as well as preparation method thereof
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CN104479854A (en) * 2014-11-27 2015-04-01 江南大学 Method for extracting peanut oil and peanut protein simultaneously
CN106118855A (en) * 2016-06-27 2016-11-16 郭迎庆 A kind of method utilizing flaxseed to prepare edible oil
CN106701312A (en) * 2017-01-08 2017-05-24 山东乐悠悠花生油科技有限公司 Aqueous enzymatic method extraction process of high-quality peanut oil
CN106753766A (en) * 2017-01-08 2017-05-31 山东乐悠悠花生油科技有限公司 A kind of method of peanut oil and peanut protein based on the low aflatoxins of aqueous enzymatic extraction
CN107586594B (en) * 2017-09-27 2021-01-01 南京工业大学 Ethanol homogenization-assisted peony seed oil extraction method
CN107586594A (en) * 2017-09-27 2018-01-16 南京工业大学 Ethanol homogenization-assisted peony seed oil extraction method
CN108641804A (en) * 2018-04-13 2018-10-12 华侨大学 A kind of method of ultrasonic wave added aqueous enzymatic extraction setose abelmoschus seed oil and protein
CN109913312A (en) * 2019-04-10 2019-06-21 北京工商大学 A kind of emulsion breakdown method that aqueous enzymatic extraction Rice oil is formed
CN110106018A (en) * 2019-05-08 2019-08-09 西藏农牧学院 A kind of open country peach peach kernel grease microcapsule and preparation method thereof
CN111234919A (en) * 2020-01-19 2020-06-05 河南农业大学 Preparation method of functional peanut oil
CN111254005A (en) * 2020-01-19 2020-06-09 河南农业大学 Preparation method of functional edible oil
CN111254005B (en) * 2020-01-19 2023-04-07 河南农业大学 Preparation method of functional edible oil
CN111234919B (en) * 2020-01-19 2023-04-07 河南农业大学 Preparation method of functional peanut oil
CN115812841A (en) * 2022-12-14 2023-03-21 中国农业科学院农产品加工研究所 Method for efficiently and synchronously separating oil and protein in peanut oil aqueous enzymatic preparation

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